CN112011009A - Based on amphiphilic Janus SiO2Nano particle stable polyacrylate emulsion and preparation method thereof - Google Patents
Based on amphiphilic Janus SiO2Nano particle stable polyacrylate emulsion and preparation method thereof Download PDFInfo
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- CN112011009A CN112011009A CN202010892454.XA CN202010892454A CN112011009A CN 112011009 A CN112011009 A CN 112011009A CN 202010892454 A CN202010892454 A CN 202010892454A CN 112011009 A CN112011009 A CN 112011009A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention relates to a method for preparing a nano-SiO based on amphiphilic Janus2The invention discloses a nano particle stable polyacrylate emulsion and a preparation method thereof, and solves the problem that amphiphilic Janus particles are not used as a surfactant and introduced into a polyacrylate emulsion system in the prior art. The invention is prepared by the following raw materials by weight: amphiphilic Janus SiO20.010-0.10 percent of particles, 6.0-8.0 percent of butyl acrylate, 5.0-6.0 percent of methyl methacrylate and initiator0.40-0.50 of ammonium sulfate and water.
Description
The technical field is as follows:
the invention relates to polyacrylate emulsion and a preparation method thereof, in particular to amphiphilic Janus SiO based emulsion2A nano particle stable polyacrylate emulsion and a preparation method thereof.
Background art:
the polyacrylate emulsion has the characteristics of excellent film forming property, good gloss and color retention, high film forming strength, high elasticity, good weather resistance, excellent aging resistance and the like, is an excellent film forming material, and is widely applied to the fields of leather, printing, coating and the like. The preparation of polyacrylate emulsions by conventional emulsion polymerization requires the addition of emulsifiers to stably nucleate the system. The addition of emulsifiers can affect the water resistance of the emulsion, thus causing certain influence on the application performance of the emulsion, and therefore, the use of traditional emulsifiers in emulsion polymerization is avoided as much as possible. Nanoparticles have attracted considerable attention from researchers due to their small size, large specific surface area, and quantum effects. Researchers have now introduced nanoparticles as emulsifiers into polyacrylate emulsion systems.
In order to improve the application performance of the particles, the concept of 'particle design' is proposed, and hydrophilic/hydrophobic Janus particles with hydrophilic groups and hydrophobic groups on two sides of the particles are designed, so that the emulsifying capacity and the interface stability of the particles are obviously improved due to the amphiphilic property similar to a surfactant. The hydrophilic/hydrophobic Janus particles are amphiphilic Janus particles, and experimental results show that compared with the particles with uniform surfaces, the adsorption energy of the amphiphilic Janus particles on an oil/water interface is 3 times that of the particles with uniform surfaces, and the emulsion can be more effectively stabilized. Therefore, the amphiphilic Janus particles can be used as a special surfactant to be introduced into a polyacrylate emulsion system. At present, no report exists that amphiphilic Janus particles are used as a special surfactant to be introduced into a polyacrylate emulsion system
Chinese patent' preparation of amphiphilic Janus SiO based on Pickering emulsion method2Preparation of nanoparticles (patent No. 201910150779.8) discloses a method for preparing amphiphilic Janus SiO2A method for preparing amphiphilic Janus SiO particles by using hydrophilic monomers of Acrylamide (AM) and Sodium Styrene Sulfonate (SSS) and hydrophobic monomers of styrene (St) and Methyl Methacrylate (MMA)2Particles.
The invention content is as follows:
the invention aims to provide a method for improving the compatibility of amphiphilic Janus SiO2The invention discloses a nano particle stable polyacrylate emulsion and a preparation method thereof, and solves the problem that amphiphilic Janus particles are not used as a surfactant and introduced into a polyacrylate emulsion system in the prior art.
In order to achieve the purpose, the invention adopts the technical scheme that:
based on amphipathic Janus SiO2The nano particle stable polyacrylate emulsion is characterized in that: the health-care food is prepared from the following raw materials in parts by weight: amphiphilic Janus SiO20.010-0.10g of particles, 6.0-8.0g of butyl acrylate, 5.0-6.0g of methyl methacrylate, 0.40-0.50g of initiator and 50g of water.
The initiator is ammonium persulfate.
Based on amphipathic Janus SiO2The preparation method of the nano particle stable polyacrylate emulsion is characterized by comprising the following steps: the method comprises the following steps:
(1) 0.010g to 0.100g of amphiphilic particles are uniformly dispersed in 30g of deionized water to form a water phase, 6.000g to 8.000g of butyl acrylate and 5.000g to 6.000g of methyl methacrylate are uniformly mixed to form an oil phase; 0.400g to 0.500g of initiator is uniformly dispersed in 20g of deionized water to form an aqueous solution;
(2) ultrasonically emulsifying an 1/3-1/2 initiator and an oil phase of 1/3-1/2 to form emulsion as a primer, and then pouring the mixed emulsion into a three-neck flask;
(3) heating in water bath to 60-80 deg.C, reacting at 300r/min, dripping the rest initiator aqueous solution and oil phase monomer, reacting for 30-60min, keeping the temperature for 2-4h, cooling to room temperature, and discharging.
Compared with the prior art, the invention has the following advantages and effects:
1. the invention adopts amphiphilic Janus nano particles as a solid emulsifier, and prepares polyacrylate emulsion through emulsion polymerization. Compared with the traditional method for preparing the polyacrylate emulsion by emulsion polymerization, the method for preparing the polyacrylate emulsion by using the amphiphilic Janus particles effectively avoids the use of the traditional emulsifier, so that the hydrophobicity and the water resistance of the emulsion after film forming are improved.
2. The invention uses amphiphilic Janus particles (0.1% -0.9%) with small dosage as a solid stabilizer, and can obtain the polyacrylate emulsion with stable particle size of about 400 nm. The method has simple preparation process and good application prospect.
3. Compared with the film formation of polyacrylate emulsion stabilized by sodium dodecyl sulfate, the invention uses amphiphilic Janus SiO2The film-forming contact angle of the emulsion prepared by taking the particles as the emulsifier is improved to 115 degrees from 45 degrees, the water absorption is reduced to 21 percent from 40 percent, and the visible light transmittance of the formed film is more than 90 percent.
The specific implementation mode is as follows:
the present invention will be described in detail with reference to specific embodiments. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. The implementation conditions used in the examples can be further adjusted according to the specific experimental environment, and the implementation conditions not mentioned are generally the conditions in routine experiments.
The invention relates to a method for preparing a nano-SiO based on amphiphilic Janus2A method for preparing a nano particle stable polyacrylate emulsion. The specific method is to use amphiphilic Janus SiO2The particles are used as a solid emulsifier to emulsify acrylic monomers, and a series of polyacrylate composite emulsion is prepared by free radical polymerization. The invention is prepared by adopting the following raw materials: amphiphilic Janus SiO20.010g-0.10g of particles, 6.0g-8.0g of butyl acrylate, 5.0g-6.0g of methyl methacrylate, 0.40g-0.50g of initiator ammonium persulfate and 50g of water.
The preparation process specifically comprises the following steps:
(1) 0.010g to 0.100g of amphiphilic particles are uniformly dispersed in 30g of deionized water to form a water phase, 6.000g to 8.000g of butyl acrylate and 5.000g to 6.000g of methyl methacrylate are uniformly mixed to form an oil phase; 0.400g to 0.500g of initiator is uniformly dispersed in 20g of deionized water to form an aqueous solution;
(2) ultrasonically emulsifying an 1/3-1/2 initiator and an oil phase of 1/3-1/2 to form emulsion as a primer, and then pouring the mixed emulsion into a three-neck flask;
(3) heating in water bath to 60-80 deg.C, reacting at 300r/min, dripping the rest initiator aqueous solution and oil phase monomer, reacting for 30-60min, keeping the temperature for 2-4h, cooling to room temperature, and discharging.
Example 1:
(1) 0.050g of amphiphilic Janus SiO2Uniformly dispersing the particles in 30g of deionized water to form a water phase, and uniformly mixing 7.200g of Butyl Acrylate (BA) and 4.800g of Methyl Methacrylate (MMA) to form an oil phase; 0.360g of initiator APS was uniformly dispersed in 20g of deionized water to form an aqueous solution.
(2) Taking out and ultrasonically emulsifying 1/3 initiator and 1/3 oil phase to form emulsion as a base, and pouring the mixed emulsion into a three-neck flask.
(3) And (3) under the conditions that the temperature is raised to 60 ℃ in a water bath and the rotating speed is 300r/min, dropwise adding the rest initiator aqueous solution and the rest oil phase monomer for 30min, then keeping the temperature for reaction for 2h, cooling to room temperature, and discharging.
Example 2:
(1) 0.100g of amphiphilic Janus SiO2Uniformly dispersing the particles in 30g of deionized water to form a water phase, and uniformly mixing 8.000g of BA and 6.000g of MMA to form an oil phase; 0.500g of initiator APS was uniformly dispersed in 20g of deionized water to form an aqueous solution.
(2) Taking out and ultrasonically emulsifying 1/3 initiator and 1/3 oil phase to form emulsion as a base, and pouring the mixed emulsion into a three-neck flask.
(3) And (3) under the conditions that the temperature is raised to 70 ℃ in a water bath and the rotating speed is 300r/min, dropwise adding the rest initiator aqueous solution and the rest oil phase monomer for 30min, then keeping the temperature for reaction for 3h, cooling to room temperature, and discharging.
Example 3:
(1) 0.010g of amphiphilic Janus SiO2Uniformly dispersing the particles in 30g of deionized water to form a water phase, and uniformly mixing 6.000g of BA and 5.000g of MMA to form an oil phase; 0.400g of initiator APS was homogeneously dispersed in 20g of deionized waterAn aqueous solution is formed.
(2) Taking out and ultrasonically emulsifying 1/3 initiator and 1/3 oil phase to form emulsion as a base, and pouring the mixed emulsion into a three-neck flask.
(3) And (3) under the conditions that the temperature is raised to 80 ℃ in a water bath and the rotating speed is 300r/min, dropwise adding the rest initiator aqueous solution and the rest oil phase monomer for 30min, then keeping the temperature for reaction for 4h, cooling to room temperature, and discharging.
The above embodiments are merely illustrative of the principles and effects of the present invention, and it will be apparent to those skilled in the art that various changes and modifications can be made without departing from the inventive concept of the present invention, and the scope of the present invention is defined by the appended claims.
Claims (3)
1. Based on amphipathic Janus SiO2The nano particle stable polyacrylate emulsion is characterized in that: the health-care food is prepared from the following raw materials in parts by weight: amphiphilic Janus SiO20.010-0.10g of particles, 6.0-8.0g of butyl acrylate, 5.0-6.0g of methyl methacrylate, 0.40-0.50g of initiator and 50g of water.
2. The amphiphilic Janus SiO-based material of claim 12The nano particle stable polyacrylate emulsion is characterized in that: the initiator is ammonium persulfate.
3. Based on amphipathic Janus SiO2The preparation method of the nano particle stable polyacrylate emulsion is characterized by comprising the following steps: the method comprises the following steps:
(1) 0.010g to 0.100g of amphiphilic particles are uniformly dispersed in 30g of deionized water to form a water phase, 6.000g to 8.000g of butyl acrylate and 5.000g to 6.000g of methyl methacrylate are uniformly mixed to form an oil phase; 0.400g to 0.500g of initiator is uniformly dispersed in 20g of deionized water to form an aqueous solution;
(2) ultrasonically emulsifying an 1/3-1/2 initiator and an oil phase of 1/3-1/2 to form emulsion as a primer, and then pouring the mixed emulsion into a three-neck flask;
(3) heating in water bath to 60-80 deg.C, reacting at 300r/min, dripping the rest initiator aqueous solution and oil phase monomer, reacting for 30-60min, keeping the temperature for 2-4h, cooling to room temperature, and discharging.
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| CN202010892454.XA CN112011009A (en) | 2020-08-31 | 2020-08-31 | Based on amphiphilic Janus SiO2Nano particle stable polyacrylate emulsion and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112724336A (en) * | 2020-12-30 | 2021-04-30 | 王海涛 | Preparation method of core-shell type polymer microsphere encapsulated with functional core material |
| CN115109179A (en) * | 2022-05-23 | 2022-09-27 | 陕西科技大学 | Based on amphipathic Janus SiO 2 Nano particle stable styrene-acrylic emulsion profile control agent and preparation method thereof |
| CN116333548A (en) * | 2023-03-31 | 2023-06-27 | 河南大学 | KH550 modified nano silicon dioxide@hydrotalcite/quadripolymer composite leather finishing agent and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105693907A (en) * | 2016-01-27 | 2016-06-22 | 上海交通大学 | Preparation method of Janus particle containing silicon dioxide with controllable particle size and asymmetrical degree |
| CN109824840A (en) * | 2019-02-28 | 2019-05-31 | 陕西科技大学 | Amphipathic Janus SiO is prepared based on Pickering emulsion method2The preparation method of nanoparticle |
-
2020
- 2020-08-31 CN CN202010892454.XA patent/CN112011009A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105693907A (en) * | 2016-01-27 | 2016-06-22 | 上海交通大学 | Preparation method of Janus particle containing silicon dioxide with controllable particle size and asymmetrical degree |
| CN109824840A (en) * | 2019-02-28 | 2019-05-31 | 陕西科技大学 | Amphipathic Janus SiO is prepared based on Pickering emulsion method2The preparation method of nanoparticle |
Non-Patent Citations (1)
| Title |
|---|
| DANGGE GAO等: "Preparation of amphiphilic Janus SiO2 particles and its application on polyacrylate emulsion", 《COLLOIDS AND SURFACES A》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112724336A (en) * | 2020-12-30 | 2021-04-30 | 王海涛 | Preparation method of core-shell type polymer microsphere encapsulated with functional core material |
| CN115109179A (en) * | 2022-05-23 | 2022-09-27 | 陕西科技大学 | Based on amphipathic Janus SiO 2 Nano particle stable styrene-acrylic emulsion profile control agent and preparation method thereof |
| CN116333548A (en) * | 2023-03-31 | 2023-06-27 | 河南大学 | KH550 modified nano silicon dioxide@hydrotalcite/quadripolymer composite leather finishing agent and preparation method thereof |
| CN116333548B (en) * | 2023-03-31 | 2024-02-02 | 河南大学 | KH550 modified nano silicon dioxide@hydrotalcite/quadripolymer composite leather finishing agent and preparation method thereof |
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